氟维司群注射液前处理及细菌内毒素检查方法研究

Study on Pre-Treatment and Bacterial Endotoxin Test of Fulvestrant Injection

目的建立氟维司群注射液细菌内毒素的检查方法。方法取样品0.5 mL,加细菌内毒素检查用水(BET用水)5 mL,2000 r/min振荡5 min后,3000 r/min离心5 min,取水相,用BET用水稀释至所需倍数系列溶液。按2020年版《中国药典(四部)》通则1143细菌内毒素检查法,分别采用凝胶法、动态显色法、动态浊度法检测样品中的内毒素,考察水萃取液(水相溶液)的干扰及内毒素回收比。结果水相溶液稀释至2倍及以上时对鲎试剂均无干扰;外加20 EU/mL内毒素时回收比均在50%~200%范围内。结论氟维司群注射液经水萃取后,采用凝胶法、动态显色法、动态浊度法进行细菌内毒素检查均可行。

Objective To establish a bacterial endotoxin test(BET)method of Fulvestrant Injection.Methods Precisely 0.5 mL of the sample was taken,5 mL of water for BET was added,then they were mixed by vortex oscillation at 2000 r/min for 5 min and centrifuged at 3000 r/min for 5 min,the aqueous phase was taken and diluted with water for BET to the desired multiple series solution.Based on the general principle 1143 bacterial endotoxin test in the Chinese Pharmacopoeia(2020 Edition,VolumeⅣ),the endotoxins in samples were tested by the gel-clot method,kinetic chromogenic assay and kinetic turbidimetric assay,and the interference of water extract(aqueous phase)and recovery ratio of endotoxins were explored.Results The aqueous phase diluted twice or more had no interfere on the tachypleus amebocyte lysate,and the recovery ratio was in the range of 50%to 200%when 20 EU/mL endotoxin was added.Conclusion It is feasible to use gel-clot method,kinetic chromogenic assay and kinetic turbidimetric assay for BET of Fulvestrant Injection after water extraction.